反应 #3721132
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06310215B1
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 29 Grams of 3-methyl-1-phenyl-2-pyrazoline-5-one and 40 ml of dimethylformamide were charged into a 200-ml three-necked flask, stirred and cooled to 0° C. in an ice-acetone bath. Then, 18.5 g of phosphorus oxychloride (POCl3) was placed in a dropping funnel, and while it was maintained at 10 to 20° C., it was dropwise added. After the addition, the mixture was heated for 1 hour, then, a reaction mixture was poured into 600 ml of ice water, and the mixture was allowed to stand for one day and night. A crystal was recovered by suction filtration, fully washed with water and dried to give the captioned compound. Yield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.). while it was maintained at 10 to 20° C. it was dropwise added After the addition the mixture was heated for 1 hour A crystal was recovered by suction filtration fully washed with water dried to give the captioned compound Yield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.)
来源 ID: ord-d6ce87e9240240ba9fb72e807c70bda7